CN106887597A - A kind of water transport plate of bore diameter gradient distribution and preparation method thereof - Google Patents

A kind of water transport plate of bore diameter gradient distribution and preparation method thereof Download PDF

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CN106887597A
CN106887597A CN201510933430.3A CN201510933430A CN106887597A CN 106887597 A CN106887597 A CN 106887597A CN 201510933430 A CN201510933430 A CN 201510933430A CN 106887597 A CN106887597 A CN 106887597A
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transport plate
water transport
water
preparation
average pore
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CN106887597B (en
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邵志刚
郭晓倩
王志强
曾亚超
瞿丽娟
衣宝廉
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8605Porous electrodes
    • H01M4/861Porous electrodes with a gradient in the porosity
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88Processes of manufacture
    • H01M4/8875Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Fuel Cell (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Inert Electrodes (AREA)

Abstract

Water transport plate the invention discloses a kind of distribution of bore diameter gradient and preparation method thereof.The water transport plate is formed by the carbon-coating stacking of 2 layers and the above, and the carbon-coating average pore size of these stackings is the structure being distributed from big to small or from small to large to opposite side average pore size from porous carbon sheet side.The method be by pore creating material, electrically conductive graphite powder, conductive carbon fibres peacekeeping resinoid bond it is well mixed after import and hot-pressing processing is carried out in mould obtain porous carbon sheet, then porous carbon sheet is carried out into high temperature graphitization treatment and hydrophilicity-imparting treatment obtains final product hydrophilic porous graphite water transport plate.The present invention can respectively regulate and control aperture, porosity and the average pore structure gradient number of graphite cake by adjusting addition type, addition and the addition number of times of pore creating material.Prepared hydrophilic porous graphite water transport plate can be average pore size multistage gradient distributed architecture.

Description

A kind of water transport plate of bore diameter gradient distribution and preparation method thereof
Technical field
The present invention relates to field of fuel cell technology, belong to the preparation method of the porous bipolar plates of fuel cell, Specially a kind of hydrophilic porous graphite water transport plate of used in proton exchange membrane fuel cell and preparation method thereof.
Background technology
Proton Exchange Membrane Fuel Cells (PEMFC) has that specific power is high with specific energy, room temperature is quickly opened The outstanding advantages such as dynamic, environmentally safe, are to get a good chance of being applied to compact power, electronic at present The electrical source of power of automobile, unmanned plane, underwater hiding-machine etc..At present, the main target of PEMFC researchs is Reduce system cost and improve battery performance and stability.And suitable water management is for realizing PEMFCs Performance optimization and stability play vital effect.In cell operation, hydrogen Generation hydrogen ion can be reduced, wherein hydrogen ion can reach cloudy with the water of anode-side by electro-osmotic effects Pole, and there is electrochemical reaction in negative electrode and electronics, oxygen, generate aqueous water.Because hydrogen ion can be taken Band hydrone, so anode-side requires supplementation with water to prevent the drying of PEM.And if aggregation Do not discharged in time in the water of cathode side, will result in battery water logging, and then prevent and suppress oxygen to arrive Up to active site surface, the performance of battery is influenceed, battery antipole is caused under serious conditions.So In order to maintain battery performance and stability it is necessary to keep the water balance in battery:The good of film should be kept Good wetting, removes aqueous water unnecessary in Catalytic Layer and diffusion layer in time again.Therefore how research is protected Suitable cell water balance is held, is had very important significance.Different from closely knit conventional panels, water transmission Plate is presented hydrophilic porous structure, and this hydrophilic duct provides the transmission channel of water.So water transport plate has Two effects:In the case of battery water shortage, the water in cooling chamber is due to the capillarity of water transport plate Air chamber can be evaporated to so as to humidification fuel air inlet;And when battery has unnecessary aqueous water, it is again Water can be discharged in cooling chamber by pressure difference.The two effects of water transport plate can effectively delay The film of electrolytic cell is dried and water logging problem, reaches suitable cell water balance.
United States Patent (USP)【US 6746982 B2】Micron-sized graphite powder is carried out into hydrophilic treated, in its table Face generation such as hydroxyl, sulfonic group hydrophilic organic group, by by the graphite powder of hydrophilic treated and conduction Graphite powder, conductive supporting carbon fiber and hot forming obtains water after macromolecule resin binding agent dry powder blend Transmission board.Konar of U.S.'s Institute of Gas Technology units et al.【US 5942347】 Hydrophilic inorganic oxide fine particle is realized bipolar plate runner with graphite powder, mixed with resin compression molding Side is hydrophilic, and hydrophilic substance absorbs negative electrode generation water and unsaturated gas is entered through water transport plate to anode Row humidification.Have by by the water transport plate that hydrophilic substance is obtained with the method for conductive materials mixing hot pressing Preferable permeable gas barrier properties, but with the increase of hydrophilic substance additive, the conduction of water transport plate Property has declined, hydrophilic substance silicone content from 0% increase to 10% when, the electric conductivity of water transport plate from 130S cm-2Fall below 50S cm-2.Cause water transport plate electric conductivity to solve to increase hydrophilic mixture The problem of decline, International Fuel Cell companies【US5840414】Propose directly in porous stone Hydrophilic metal oxide SnO is generated in the hole of black plate2Method prepare water transport plate, because of porous stone The black plate conductive network of itself, influence will not be produced after generating hydrophilic substance in hole on the electric conductivity of plate, The electric conductivity of plate is effectively improved.Because aqueous water is more easy in the small hydrophilic pores of entrance aperture, institute So that in order to increase draining and the humidifying capacity of water transport plate, researchers are devoted to preparing water transport plate Into the structure of bore diameter gradient distribution.Australian Patent【389020】Devise a kind of PEM Fuel cell is stacked structure, and it is provided passive cold using the water cooling plate component in gradient aperture But agent and water management are controlled.There are the cooling water cavity for being carved with flow field, water cavity two in the middle of water cooling plate component Side has different apertures, using the side of small-bore and minimal thickness as anode-side, greatly large aperture and thickness Degree side is used as adjacent cathode side.When cell cathode accumulates aqueous water, the cooling board component will Unnecessary aqueous water is absorbed to cooling chamber, and because the plate near anode-side is thinner and aperture is smaller, Because capillary force, the water in cooling water cavity can enter anode-side to gas through water cooling plate component Body is humidified.Although porous plate prepared by this method possesses good electric conductivity, this water cooling Plate is obtained by graphite machining.
The content of the invention
It is an object of the invention to provide one kind prepare the hydrophilic porous graphite water transport plate of fuel cell and its Preparation method, it is ensured that it has the characteristics such as good permeable, choke, electrical conductivity and compression strength.
To achieve these goals, the technical solution adopted by the present invention is:
1) it is placed in after being well mixed pore creating material, electrically conductive graphite powder, conductive carbon fibres peacekeeping resinoid bond In mould, change pore creating material species or addition and repeat the above steps, wherein number of repetition is n Secondary (n >=0, n is integer), hot forming treatment is carried out by the powder in mould, is removed pore creating material and is obtained final product Porous carbon sheet (works as n=0, porous carbon sheet does not form average pore size gradient distributed architecture;Work as n>0, and Porous carbon sheet can form average pore size n+1 grades of graded structure during every layer of addition different pore creating material, N+1 grades of described graded structure is formed by the carbon-coating stacking of 2 layers and the above, these stackings Carbon-coating average pore size is to divide from big to small or from small to large to opposite side average pore size from porous carbon sheet side The structure of cloth);
2) hot pressing carbon plate is obtained into porous graphite cake after 2000-3500 DEG C of high temperature graphitization processes 1-3h;
3) porous graphite plate is placed in butyl titanate solution, wherein solvent is water and ethanol, in vacuum Spend to carry out vacuumize process 10-60min under 0.02-0.1MPa, then take out drying, be finally placed in 400-500 DEG C of high-temperature roasting treatment 2-5h in Muffle furnace.
The ratio of pore creating material, electrically conductive graphite powder, reinforcing fiber and resin glue described in step (1) It is 5-30wt%:50-75wt%:5-15wt%:10-20wt%, four sums are 100wt%, hot pressing Pressure is 1-10MPa, and hot pressing temperature is 100-250 DEG C, and hot pressing time is 10-60min;
Pore creating material described in step (1) is (NH4)2C2O4、NH4NO3、NH4HCO3、(NH4)2SO4、 One or two or more kinds in NaCl, KCl.
Electrically conductive graphite powder described in step (1) is one kind of KS75, K150 or expanded graphite or two kinds More than, its particle diameter is 1-60 μm.
Reinforcing fiber described in step (1) for the one kind in carbon fiber, graphite fibre, glass fibre or More than two kinds, a diameter of 1-15 μm, draw ratio is 10-50.
Resin glue described in step (1) is thermoplastic resin, and thermoplastic resin is polyethylene, gathers One kind of propylene, polyphenylene sulfide, polyether sulfone, thermoplastic phenolic resin and polyethylene terephthalate Or more than two kinds.
Step (2) the high temperature graphitization treatment temperature is 2000-3500 DEG C, and process time is 1-3h.
Butyl titanate solution concentration described in step (3) is 0.01-1mol L-1, solvent is water and ethanol Mixed liquor, the volume ratio of solvent reclaimed water and ethanol is 0.1-2.
Advantages of the present invention is mainly reflected in:
1. the present invention can be by adjusting the addition type of pore creating material and the hole of addition Effective Regulation graphite cake Footpath and porosity;
2. the hydrophilic porous graphite water transport plate for preparing can be average pore size multistage gradient distributed architecture.
Brief description of the drawings
The cross-sectional view of water transport plate when Fig. 1 is n=0;
The cross-sectional view of water transport plate when Fig. 2 is n=1;
The cross-sectional view of water transport plate when Fig. 3 is n=2;
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1
By pore creating material NH4NO3, electrically conductive graphite powder KS150 (35 μm of particle diameter), carbon fiber (diameter It it is 11 μm, 5) draw ratio is and carries out hot pressing with mould after adhesive phenolic resin is well mixed, respectively Component ratio is 10%:70%:10%:10%, hot pressing temperature is 150 DEG C, and pressure is 4MPa, heat The pressure time is 40min, obtains final product porous carbon sheet of the aperture without gradient-structure, and aperture schematic diagram is shown in Fig. 1.It is many The thickness of hole carbon plate is 1mm, and average pore size is 2.5 μm, and porosity is 22%.Again by porous carbon Plate carries out high temperature graphitization and processes to obtain porous graphite cake, and treatment temperature is 2000 DEG C, and process time is 2h. The average pore size of porous graphite plate is 2.3 μm, and porosity is 26%.Porous graphite plate is placed in concentration It is 0.05mol L-1Vacuum 0.03MPa is used in butyl titanate solution (volume ratio of water and ethanol is 0.5) Vacuumize process 30min, hydrophilic porous graphite water transport plate is obtained final product after 500 DEG C of roasting 3h.Gained water Transmission board average pore size is 1.9 μm, and porosity is 21%.
Embodiment 2
By pore creating material NaCl, electrically conductive graphite powder KS75 (50 μm of particle diameter), carbon fiber (a diameter of 17 μm, 10) draw ratio is and pours into mould middle berth after binding agent melamine formaldehyde resin is well mixed Flat, each component ratio is 10%:70%:10%:10%, then uniformly poured on above-mentioned powder surface and make Hole agent (NH4)2C2O4, electrically conductive graphite powder KS75 (50 μm of particle diameter), graphite fibre (a diameter of 17 μm, Draw ratio is mixed-powder 10) with binding agent melamine formaldehyde resin, and the ratio of each component is 20%:60%:10%:10%, hot pressing is then carried out, hot pressing temperature is 210 DEG C, and pressure is 2MPa, Time is 20min.Above-mentioned hot pressing carbon plate is placed in 30min in the aqueous solution and removes pore creating material NaCl, obtained To the porous carbon sheets of two grades of average pore size gradients distribution, aperture schematic diagram is shown in Fig. 3.By (NH4)2C2O4 One layer of pore-creating is defined as 1 layer, and NaCl's is 2 layers.The thickness that 1 layer of porous carbon sheet is 0.5mm, Average pore size is 1.7 μm, and 2 layers of thickness is 0.5mm, and average pore size is 4.4 μm, overall porosity It is 30%.Porous carbon sheet is carried out into high temperature graphitization again and processes to obtain porous graphite cake, hot-press method and bar Part is same as Example 1.The average pore size of 1 layer of porous graphite plate is 1.9 μm, 2 layers of average hole Footpath is 3.9 μm, and overall porosity is 37%.Porous graphite plate is placed in concentration for 0.2mol L-1Metatitanic acid Vacuum 0.05MPa vacuumize process 20min are used in butyl acetate solution (volume ratio of water and ethanol is 0.2), Hydrophilic porous graphite water transport plate is obtained after 450 DEG C of roasting 2h.1 layer of average pore size of gained water transport plate be 1.7 μm, 2 layers of average pore size is 3.4 μm, and overall porosity is 34%.
Embodiment 3
By pore creating material NaCl, electrically conductive graphite powder KS75 (50 μm of particle diameter), carbon fiber (a diameter of 15 μm, Draw ratio is to pour into mould to pave after 10) being well mixed with adhesive phenolic resin, each component ratio It is 10%:70%:10%:10%, then uniformly pour into pore creating material NH on above-mentioned powder surface4NO3, lead Calcium carbide ink powder KS75 (50 μm of particle diameter), glass fibre (a diameter of 15 μm, draw ratio be 10) and The mixed-powder of adhesive phenolic resin, the ratio of each component is 15%:65%:8%:12% again upper State powder surface and uniformly pour into pore creating material (NH4)2C2O4, electrically conductive graphite powder KS75 (50 μm of particle diameter), (a diameter of 15 μm, draw ratio is mixed-powder 10) with adhesive phenolic resin, each group to carbon fiber The ratio divided is 20%:60%:10%:10%, hot pressing is then carried out, hot pressing temperature is 190 DEG C, Pressure is 2MPa, and the time is 20min.Above-mentioned hot pressing carbon plate is placed in into 30min in the aqueous solution to remove Pore creating material NaCl, obtains the porous carbon sheet of three-level average pore size gradient distribution, and aperture schematic diagram is shown in Fig. 3. By (NH4)2C2O4One layer of pore-creating is defined as 1 layer, NH4NO3Be 2 layers, NaCl's is 3 layers. The thickness that 1 layer of porous carbon sheet is 0.5mm, and average pore size is 1.7 μm, and 2 layers of thickness is 0.5mm, Average pore size is 2.8 μm, and 3 layers of thickness is 0.5mm, and average pore size is 4.4 μm, overall porosity It is 27%.Porous carbon sheet is carried out into high temperature graphitization again and processes to obtain porous graphite cake, hot-press method and bar Part is same as Example 1.The average pore size of 1 layer of porous graphite plate is 1.9 μm, 2 layers of average hole Footpath is 2.7 μm, and 3 layers of average pore size is 3.9 μm, and overall porosity is 35%.Porous graphite plate is put In concentration be 0.1mol L-1Vacuum is used in butyl titanate solution (volume ratio of water and ethanol is 1) 0.08MPa vacuumize processs 20min, hydrophilic porous graphite water transport plate is obtained after 450 DEG C of roasting 2h. 1 layer of average pore size of gained water transport plate is 1.7 μm, and 2 layers of average pore size are 2.3 μm, 3 layers average Aperture is 3.4 μm, and overall porosity is 29%.
Table 1 is the physical property of the water transport plate of each embodiment.
The method of testing of contact angle is in water transport plate surface, then with connecing by the deionized water drop of 3 μ l The analysis of feeler tester obtains final product contact angle values.Hydrophilic pores ratio method of testing is first to weigh water transport plate Dry weight, then plate is placed in 80 DEG C of hot water impregnates 8h, wipe remained on surface aqueous water with filter paper after taking-up And weigh, obtain final product hydrophilic pore volume;The plate soaked through water is placed in after drying 24h in vacuum drying chamber Above-mentioned subsequent step is placed in 80 DEG C of n-decanes and repeated, total open volume is obtained final product, by hydrophilic pore volume It is divided by with total open volume and obtains final product hydrophilic pores ratio.
Table 2 is the permeable gas barrier properties of the water transport plate of each embodiment.
Permeable method for testing pressure is the side for introducing the water into water transport plate, and the opposite side of plate exposes In atmosphere, then water side is pressurizeed, the pressure when water droplet occurs in the air side of plate is Water pressure;Pressure in bubbles method of testing is in the side of the above-mentioned water transport plate by permeable pressure test Pressurizeed with nitrogen, the pressure as pressure in bubbles when the opposite side of plate has bubble to occur.Permeable measurement Method for testing is the both sides for adding water to plate, and the wherein side to plate is pressurizeed, the pressure of fixed side It is 0.02MPa, the reduction speed of pressure side water is the penetration by liquid water flux of water transport plate.

Claims (10)

1. the water transport plate that a kind of average pore size gradient is distributed, it is characterised in that:By 2 layers or 3 layers with On carbon-coating stacking form, these stacking carbon-coating average pore sizes be from porous carbon sheet side to opposite side The structure that average pore size is distributed from big to small or from small to large.
2. water transport plate according to claim 1, it is characterised in that:The water transport plate plane electricity Resistance rate is 1-5m Ω cm, and bending strength is 5-50MP, and permeable pressure is 0-0.03MPa, and bubble point is 0.05-0.2MPa, contact angle is 5 ° -85 °, and thickness is 0.5-7mm, and average pore size is 0.1-20 μm, Porosity is 5%-50%, and on the basis of all of hole of water transport plate, hydrophilic pores ratio is 50%-100%.
3. the preparation method of the water transport plate described in a kind of claim 1 or 2, it is characterised in that:Bag Include following steps:
(1) pore creating material, electrically conductive graphite powder, conductive carbon fibres peacekeeping resinoid bond are well mixed rearmounted In mould, change the species or addition of pore creating material and repeat the above steps, wherein number of repetition It is n times (n >=0, n is integer) that the powder in mould is carried out into hot forming treatment, removes pore creating material Obtain final product porous carbon sheet;
(2) porous carbon sheet that hot pressing is formed is processed into obtain porous graphite cake by high temperature graphitization;
(3) porous graphite plate is placed in butyl titanate solution, it is 0.02-0.1MPa to carry out in vacuum Lower vacuumize process 10-60min, then takes out drying, is finally placed in 400-500 DEG C high in Muffle furnace Warm calcination process 2-5h.
4. the preparation method of water transport plate according to claim 3, it is characterised in that:Step (1) The ratio of the pore creating material, electrically conductive graphite powder, reinforcing fiber and resin glue is 5-30wt%: 50-75wt%:5-15wt%:10-20wt%;In the hot pressing, pressure is 1-10MPa, temperature It it is 100-250 DEG C, the time is 10-60min.
5. the preparation method of water transport plate according to claim 3, it is characterised in that:Step (1) Described pore creating material is (NH4)2C2O4、NH4NO3、NH4HCO3、(NH4)2SO4, NaCl or KCl In one or two or more kinds.
6. the preparation method of water transport plate according to claim 3, it is characterised in that:Step (1) Described electrically conductive graphite powder is one or two or more kinds in KS75, K150 or expanded graphite, its grain Footpath is 1-60 μm.
7. the preparation method of water transport plate according to claim 3, it is characterised in that:Step (1) Described conductive fiber is one or two or more kinds of carbon fiber, graphite fibre or glass fibre, diameter It it is 1-15 μm, draw ratio is 10-50.
8. the preparation method of water transport plate according to claim 3, it is characterised in that:Step (1) Described resin glue is thermoplastic resin, and above-mentioned thermoplastic resin is polyethylene, polypropylene, gathers One kind of diphenyl sulfide, polyether sulfone, thermoplastic phenolic resin or polyethylene terephthalate or two kinds with On.
9. the preparation method of water transport plate according to claim 3, it is characterised in that:Step (2) The high temperature graphitization treatment temperature is 2000-3500 DEG C, and process time is 1-3h.
10. the preparation method of water transport plate according to claim 3, it is characterised in that:Step (3) Described butyl titanate solution concentration is 0.01-1mol L-1, solvent is the mixed liquor of water and ethanol, solvent The volume ratio of reclaimed water and ethanol is 0.1-2.
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CN111082072A (en) * 2019-12-31 2020-04-28 上海神力科技有限公司 Gas diffusion layer for fuel cell and preparation method thereof
CN113977025A (en) * 2020-12-04 2022-01-28 中国电器科学研究院股份有限公司 Method for preparing large-gap soldered joint
WO2022252389A1 (en) * 2021-05-31 2022-12-08 东华大学 Gas diffusion layer for proton exchange membrane fuel cell and preparation method thereof
CN116364948A (en) * 2023-03-24 2023-06-30 一汽解放汽车有限公司 Pore-diameter gradient cathode catalytic layer and preparation method and application thereof
CN117374313A (en) * 2023-10-20 2024-01-09 苏州大学 Gas diffusion layer of proton exchange membrane fuel cell and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN111082072A (en) * 2019-12-31 2020-04-28 上海神力科技有限公司 Gas diffusion layer for fuel cell and preparation method thereof
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CN117374313A (en) * 2023-10-20 2024-01-09 苏州大学 Gas diffusion layer of proton exchange membrane fuel cell and preparation method and application thereof

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